Hydrochloric Acid → HCID 22717663, Verbindung

HRID 1582542Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1582542
[NH2:1][C:2]1[S:3][C:4]([I:11])=[C:5]([C:7]([F:10])([F:9])[F:8])[N:6]=1.[F:12][C:13]([F:28])([F:27])[C:14]1[CH:15]=[C:16]([CH:20]=[C:21]([C:23]([F:26])([F:25])[F:24])[CH:22]=1)[C:17](Cl)=[O:18].Cl>N1C=CC=CC=1>[I:11][C:4]1[S:3][C:2]([NH:1][C:17](=[O:18])[C:16]2[CH:20]=[C:21]([C:23]([F:24])([F:25])[F:26])[CH:22]=[C:14]([C:13]([F:12])([F:27])[F:28])[CH:15]=2)=[N:6][C:5]=1[C:7]([F:10])([F:8])[F:9]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 1018563,5-Bis(trifluoromethyl)benzoyl chlorideHCID 227176715-Iodo-4-(trifluoromethyl)-1,3-thiazol-2-amine

Produkt 1

HCID 22717663HCID 22717663, VerbindungAusbeute 71,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

2-Amino-5-iodo-4-trifluoromethylthiazole (1.0 g) was dissolved in pyridine (2 ml) and 3,5-bis-trifluoromethylbenzoylchloride (0.95 g) was added at room temperature with stirring. The mixture was stirred for 6 hr at room temperature. The mixture was poured into ice water and acidified with aqueous hydrochloric acid then extracted with chloroform. The chloroform layer was dried over magnesium sulfate and the solvent was removed under reduced pressure. The solid thus obtained was recrystallized from methanol to give N-(5-iodo-4-trifluoromethylthiazol-2-yl)-3,5-bis-trifluoromethylbenzamide (1.3 g), m. p. 172-173° C.

Aufarbeitung

  1. stirringThe mixture was stirred for 6 hr at room temperature
  2. extractionthen extracted with chloroform
  3. dry with materialThe chloroform layer was dried over magnesium sulfate
  4. customthe solvent was removed under reduced pressure
  5. customThe solid thus obtained
  6. customwas recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-415e641e0a1143ae9382700f88385343
Quelldatensatz
uspto-grants-2004_05
Patentnummer
US06737382B1

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